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Water → 5-Chloro-2,3-dihydroxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 5-Chloro-2-hydroxy-3-methoxybenzaldehyde | HCID 5151086 | — |
| 溶媒 | Hydrogen Bromide | HCID 260 | — |
| 生成物 | 5-Chloro-2,3-dihydroxybenzaldehyde | HCID 21924862 | 32.5% |
反応手順
5-Chloro-2-hydroxy-3-methoxy-benzaldehyde (see J. Org. Chem. 56; 1991; 5451; 20.0 g, 107 mmol) was suspended in hydrobromic acid (100 mL of 47% in water). The mixture was refluxed for 6 h and then cooled to room temperature before dilution with water (300 mL). The formed precipitate was collected by filtration and then washed with water. After air drying, the solid material was purified by soaking with CH2Cl2 (4×150 mL). There was obtained 6.0 g (32%) of 5-chloro-2,3-dihydroxybenzaldehyde as a solid. 1H NMR (300 MHz, CDCl3): 5.7 (s, 1H), 7.1 (d, 1H), 7.2 (d, 1H), 9.8 (s, 1H), 11.0 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07402581B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-06596c0af36c409eb8256a89b15ca4b6 |
| 出典メモ | uspto-grants-2008_07 |